Lamellar phases containing vanadium oxide: synthesis, characterization and application of the adsorption of phenol from aqueous solutions

Lamellar phases of the general formula [CnH(2n+1)N(CH3)3]VO3 (n = 14, 16, 18) have been prepared by an ion-exchange/precipitation reaction of alkyltrimethylammonium surfactants and NaVO3 in an aqueous medium at room temperature. The phases were characterized by powder X-ray diffraction, transmission electron microscopy, infrared spectroscopy, thermogravimetric analysis and differential scanning calorimetry. The data support a proposed crystal structure model in which single arrays of the one-dimensional chains of oligomers {(VO3)n}(n-) that may be generated from the starting material NaVO3 fragmented by the hydration during the dissolution into water and the surfactants layers alternate. The alkyl chains of the surfactants in these materials are arranged as monolayers or deeply penetrate into the interlayer region with a tilt angle of 37 degrees. The phenol adsorption in aqueous solution on a representative lamellar phase was investigated. The data being fitted to Langmuir Isotherms and a maximum adsorption capacity calculated from the Langmuir equation to be 178.6 mg of phenol/g for [C16H33N(CH3)3]VO3 have been obtained. The effect of pH on the adsorption and desorption of phenol has also been studied. Acetone solution of 20% is the best eluent for desorption of phenol from the loaded adsorbent with a desorption efficiency of 90.8%.     

Synthesis and characterization maleate-alumoxane nanoparticles for removal of reactive yellow 84 dye from aqueous solution

Maleate-alumoxane nanoparticles (Mal-A) were synthesized from boehmite and applied for adsorption of an azo dye (Reactive Yellow 84) from aqueous solution. Its adsorption capacity was compared with three types of carboxylate alumoxane nanoparticles synthesized from boehmite including salicylate alumoxane (Sal-A), para-aminobenzoate alumoxane (Pab-A) and fumarate alumoxane (Fum-A). The characterizations of prepared materials were analyzed using FTIR, SEM, X-ray diffraction and BET measurements. Among utilized alumoxanes at natural pH, the adsorption capacity of Mal-A was 45, 67, 116 and 215% higher than that of Fum-A, Boehmite, Pab-A, Sal-A nanoparticles, respectively. Response surface methodology (RSM) using Box-Behnken design of experiment was employed to investigate the influence of pH, initial concentration of dye and adsorbent dosage on dye removal efficiency of Mal-A. Box-cox transformation was chosen to improve model adequately and a good prediction (R²: 0.998) was achieved. Under optimum condition, i.e., pH: 4.3, dye concentration: 151.5 mg/L and adsorbent dosage: 1.2 g/L, the adsorption capacity and dye removal efficiency were obtained 130.6 mg/g and 99.2%, respectively. The kinetics and equilibrium data were perfectly represented with linear pseudo-second-order and linear Langmuir isotherm models, respectively.     

Na0.5Li0.5CoO2 nanopowders: Facile synthesis,characterization and their application for the removal of methylene blue dye from aqueous solution

In this paper, delafossite-type Na_0.5Li_0.5CoO₂ nanoparticles (NPs) with an average particle size of 50 nm were successfully synthesized by sol–gel method. Prepared NPs were characterized by differential thermal analysis, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and scanning tunneling microscopy. The nanoparticles showed the excellent adsorption properties towards methylene blue dye (MBD) as a reactive dye. The kinetics of removal of MBD in aqueous solutions was studied in a series of experiments which were varied in the amount of NPs, contact time, pH, and temperature. The experimental data were fitted very well in the pseudo-second order kinetic model and the Freundlich adsorption isotherm model. 92% of dye was successfully removed in 10 min using 0.02 g Na_0.5Li_0.5CoO₂ NPs in a pH = 11. Thermodynamic study indicates that the adsorption of MBD is feasible, and spontaneous in nature.     

Microwave-assisted synthesis and characterization of tin oxide nanoparticles

Tin oxide nanoplatelets (SnO) and nanoparticles (SnO₂) were prepared by microwave assisted technique with an operating frequency of 2.45 GHz. This technique permits to produce gram quantity of homogeneous nanoparticles in just 10 min. The crystalline size was evaluated from XRD and found to range from 26 to 34 nm. SEM and TEM analyses showed that the nanoparticles present a platelet-like shaped particle or, a pseudo spherical morphology, after calcination at moderate temperature during which the phase transformation from SnO to SnO₂ takes place. Additional FT-IR, density and resistivity measurements were also presented.     

Towards carbon-free flame spray synthesis of homogeneous oxide nanoparticles from aqueous solutions

Flame-assisted spray pyrolysis (FASP) is a versatile process for synthesis of nanoparticles from a broad choice of precursors and solvents. Water is an attractive solvent particularly for inexpensive inorganic precursors (e.g. metal nitrates) as it can effectively reduce the process cost. Furthermore when water usage is combined with a carbon-free fuel (e.g. H₂), nanoparticles can be made without forming CO₂. Here such a FASP process is explored for synthesis of Bi₂O₃ and other oxide nanoparticles from aqueous precursor solutions. The flame temperature was measured by FTIR emission–transmission spectroscopy while powders were characterized by X-ray diffraction and N₂ adsorption. At low FASP fuel gas (H₂ or C₂H₂) flow rates or process temperatures, product powders had a bimodal crystal size distribution. Its large and small modes were made by droplet- and gas-to-particle conversion, respectively. Homogeneous Bi₂O₃ and CeO₂ powders were obtained for sufficiently high flow rates of either C₂H₂ or H₂. Prolonged high temperature residence times promoted precursor evaporation from the spray droplets and yielded homogeneous nanostructured powders by gas-to-particle conversion. In contrast, FASP of aqueous solutions of aluminum nitrate yielded rather large particles by droplet-to-particle conversion at all fuel flows investigated.     

Flower-shaped gold nanoparticles: synthesis, characterization and their application as SERS-active tags inside living cells

The detection of Raman signals inside living cells is a topic of great interest in the study of cell biology mechanisms and for diagnostic and therapeutic applications. This work presents the synthesis and characterization of flower-shaped gold nanoparticles and demonstrates their applicability as SERS-active tags for cellular spectral detection. The particles were synthesized by a facile, rapid new route that uses ascorbic acid as a reducing agent of gold salt. Two triarylmethane dyes which are widely used as biological stains, namely malachite green oxalate and basic fuchsin, were used as Raman-active molecules and the polymer mPEG-SH as capping material. The as-prepared SERS-active nanoparticles were tested on a human retinal pigment epithelial cell line and found to present a low level of cytotoxicity and high chemical stability together with SERS sensitivity down to picomolar particle concentrations.     

Hydrothermal synthesis of zirconium oxide nanoparticles and its characterization

The paper presents the preparation and investigations of zirconium oxide (ZrO₂) nanoparticles that were synthesized by hydrothermal method. The products were characterized by means of powder X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-absorption spectroscopy and photoluminescence (PL) spectroscopy. The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The spherical shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR and Raman spectrum ascertained the strong presence of ZrO₂ nanoparticles. The optical properties were obtained from UV–visible absorption spectrum and also PL emission spectrum. The dielectric constant and the dielectric loss were measured as a function of frequency and temperature.     

Synthesis and photochemical performance of CdS nanoparticles photocatalysts for photodegradation of organic dye

Large scale CdS nanoparticles are synthesized by a facile and effective route. The as-prepared CdS product was characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electronmicroscopy, photoluminescence spectroscopy, X-ray photoelectron spectroscopy and UV–Vis diffuse reflectance spectroscopy. The CdS nanoparticles showed higher photocatalytic activity for the discoloration of methyl orange under UV light irradiation for 90 min. Significantly, the stability and recycling of the photocatalyst was also investigated. This study may provide a new insight into the design and prepared of visible-light photocatalytic materials.     

Preparation and characterization of bio-functionalized iron oxide nanoparticles for biomedical application

Amine modified iron oxide (Fe₃O₄) nanoparticles were synthesized by thermal decomposition method and were further used to bio-functionalize by grafting of N-hydroxysuccinimide (NHS) ester of folate and ethylenediaminetetraacetate (EDTA). Fe₃O₄ nanoparticles of ~ 22 nm were confirmed from X-ray diffraction (XRD) and transmission electron microscopy (TEM) studies. FT-IR studies indicated two bands at 1515 cm^− 1and 1646 cm^− 1, which can be attributed to carboxylic group and the amide linkage respectively, revealing the conjugation of folate with Fe₃O₄. The conjugation of the chelating agent showed strong C=O stretch and Fe-O vibrations at 1647 and 588 cm^− 1 respectively. The value of saturation magnetization for Fe₃O₄ nanoparticles was found to be 88 emu/g, which further reduced to 18 and 32% upon functionalization with EDTA and NHS ester folate, respectively. These amine modified Fe₃O₄ nanoparticles can also be functionalized with other bifunctional chelators, such as amino acids based diethylene triamine pentaacetic acid (DTPA), and thus find potential applications in radio-labeling, biosensors and cancer detection, etc.     

Tri-doped co-annealed zinc oxide semi-conductor synthesis and characterization: photodegradation of dyes and gas sensing applications

Despite the fact that much of the research has been performed on ZnO-based nanoparticles, still a lot of work is unexplored. The synthesis and characterization of the ZnO nanorods have been co-annealed using a simple combustion method and used for gas sensor and photocatalytic degradations applications. Herein pure and In, Sn and Sb tri-dopants were used, i.e. 0.5 at.wt% 1.0 at.wt% and 1.5 at.wt%, while their effects co-annealed on glass substrate at different temperatures at 500 °C and 1100° have been studied. These samples were coated onto the chosen substrate using spin coating technique. Crystallite scale was measured to the range of 30–50 nm. At such temperatures, the grain size measured for the samples was in range of 50–70 nm. This showed that the prepared nanorods are well crystalline and have strong optical properties to handle. Studies of X-ray diffraction showed the influential point (101). These coated samples designed for nitrogen gas sensing have been tested for the development of smart and functional instruments. Furthermore, it was observed that the samples prepared at higher temperatures exhibit better recovery and better reaction time. Valance ion process explains the gas sensors fast reaction and long recovery time. Thus prepared ZnO nanoparticles have photocatalytic degradation (99.86%) only in 55 min. We observed optimum exposure at an operating temperature of 105 °C. It is notable that morphology of susceptible layer nanoparticles is preserved based on different tri-doping concentrations. The concentration of T2-ZnO nanoparticles for photodegradation of the DR-31 dye and NO₂ gas sensing applications were 1.0 at.wt%

     

Facile synthesis of magnetic iron oxide nanoparticles and their characterization

Magnetic iron oxide nanoparticles are synthesized by suitable modification of the standard synthetic procedure without use of inert atmosphere and at room temperature. The facile synthesis procedure can be easily scaled up and is of important from industrial point of view for the commercial large scale production of magnetic iron oxide nanoparticles. The synthesized nanoparticles were characterized by thermal, dynamic light scattering, scanning electron microscopy and transmission electron microscopy analyses.     

Novel photothermal-responsive sandwich-structured mesoporous silica nanoparticles: synthesis,characterization, and application for controlled drug delivery

Novel thermal nanoparticles [hollow mesoporous silica nanospheres (HMSNs)–poly (N-isopropyl acrylamide-acrylic acid) PNIPAM-AA] were developed with Ag nanoparticles (AgNps) as the core, mesoporous silica nanoparticles as the layer, and thermally responsive polymers PNIPAM-AA as the shell. The AgNps had good photothermal effects, PNIPAM-AA was responsive to temperature, the combination of AgNps and PNIPAM-AA could be used as a photothermal-responsive switch for drug release, and HMSNs greatly increased the drug loading of the carrier. The samples were characterized by means of scanning electron microscopy, transmission electron microscopy, N₂ adsorption–desorption, thermogravimetric analysis, Fourier transform infrared spectroscopy, and UV–Vis absorption spectra. The results showed that Ag@HMSN nanoparticles possessed a uniform diameter (330 nm), high specific surface area (822.45 m²/g), and mesoporous pore size (2.75 nm). Using ibuprofen (IBU) as a model drug, the release process was monitored under in vitro conditions to investigate its release characteristics at different temperatures. The results showed that the nanoparticles had a significant regulatory effect on IBU release.

Graphical abstract

     

Green synthesis of copper oxide nanoparticles and its effective applications in Biginelli reaction,BTB photodegradation and antibacterial activity

Metal/metal oxide nanoparticles have gained much attention in the field of organic catalysis and photocatalysis reactions for development of greener methodology. In the present work, copper oxide nanoparticles (CuO NPs) were synthesized by a greener route using Cordia sebestena (C. sebestena) flower aqueous extract. The nanoparticles were evaluated for their catalytic efficiency. The green synthesized CuO NPs were characterized using various analytical studies. A UV–Visible spectrum with peak at 267?nm and the peaks in their FT-IR spectrum at 431 and 542?cm^?1 showed reduction by the plant metabolites. FESEM-EDX analysis of CuO NPs shows an agglomerated spherical shape with signatures of Cu and O and XRD reveals characteristic crystallinity. TEM and DLS analyses showed particle size between 20 and 35?nm and TEM-SAED pattern ensured crystallinity. A Zeta potential of ?26?mV demonstrates moderate stability. The CuO NPs acted as a catalyst in the Biginelli reaction to produce 3,4-dihydropyrimidinones rapidly and at high yield. The NPs also degraded bromothymol blue (BTB) by photocatalysis with hydrogen peroxide. 100% dye removal efficiency was achieved by 3?h exposure of BTB to natural sunlight inferring it as economy, ecofriendly and effective catalyst. This finding illustrates that the NPs could be used in photolysis to remove water pollutants. Moreover, the biological significance of green synthesized CuO NPs was assessed by antibacterial activity against selected pathogenic bacterial organisms.     

Zinc oxide micro- and nanoparticles: Synthesis, structure and optical properties

Zinc oxide (ZnO) spherical nanoparticles (SNPs) and bitter-melon-like (BML) microparticles were synthesized by a hydrothermal route using a zinc (Zn) plate as a source and substrate at various synthesis conditions. The structural analysis confirmed the formation of ZnO with hexagonal wurtzite phase on the hexagonal Zn substrate with growth of the ZnO microparticles along the [1 0 1] direction. The UV-vis absorption spectra of the ZnO microparticles indicated absorption peaks in the UV region which can be attributed to the band gap of ZnO. The room temperature photoluminescence (PL) of the ZnO microparticles exhibited a broad emission band, which is fitted with four Gaussian peaks and were assigned to transitions involving free excitons and various defect centers. The growth model for the formation of ZnO micro- and nanoparticles is presented.     

Adsorbents made from textile scraps: preparation,characterization and application for removal of reactive dye

Textile scraps from the clothing industry were used to prepare a low-cost adsorbent to remove anionic dye from textile effluents. Adsorbents were prepared through pyrolysis and chemical activation with K₂CO₃. These samples were characterized through thermogravimetric analysis, scanning electron microscopy, N₂ adsorption/desorption isotherms, Fourier transform infrared spectroscopy, point of zero charge, isoelectric point, elemental composition and proximate analysis. Batch kinetic experiments and adsorption isotherm modeling were conducted in different conditions. The surface properties of the adsorbents were significantly influenced by the activation process. The highest BET surface area (S_BET = 358.55 m² g^?1) was attributed to the sample with chemical treatment. The results indicate that activation process raised 700% the adsorption capacity. The adsorption was strongly dependent on the pH. For the activated adsorbent, 6 g L^?1 was sufficient for the complete removal of 40 mg L^?1 Reactive Black 5 (RB5) solution. The monolayer capacity was up to 10.3 mg g^?1 and was higher than a commercial activated carbon commonly used in textile sector, which was 9.7 mg g^?1.     

Preparation, characterization and adsorption properties of chitosan nanoparticles for eosin Y as a model anionic dye

The present study dealt with the adsorption of eosin Y, as a model anionic dye, from aqueous solution using chitosan nanoparticles prepared by the ionic gelation between chitosan and tripolyphosphate. The nanoparticles were characterized by atomic force microscopy (AFM), size and zeta potential analysis. A batch system was applied to study the adsorption of eosin Y from aqueous solution by chitosan nanoparticles. The results showed that the adsorption of eosin Y on chitosan nanoparticles was affected by contact time, eosin Y concentration, pH and temperature. Experimental data followed Langmuir isotherm model and the adsorption capacity was found to be 3.333 g/g. The adsorption process was endothermic in nature with an enthalpy change (DeltaH) of 16.7 kJ/mol at 20-50 degrees C. The optimum pH value for eosin Y removal was found to be 2-6. The dye was desorbed from the chitosan nanoparticles by increasing the pH of the solution.     

Preparation of iron oxide nanoparticles by microwave synthesis and their characterization

In this study production of fine particle Fe2O3 via microwave processing of Fe(NO3)3.nH2O followed by low temperature annealing was reported. XRD was used to characterize the structural properties of nanoparticles. Approximate particle sizes were between 3-13 nm according to Scherrer's equation. Single point BET measurement results also show that samples have large surface area and they are nanometer sized particles. TEM study was conducted to examine the structure of the nanoparticles. TEM figure is in good agreement with the results obtained from Scherrer's equation using XRD spectra. In order to characterize the magnetic properties of the nanoparticles VSM (Vibrating Sample Magnetometer) was used. From these results it can be concluded that the sample containing only maghemite phase exhibits superparamagnetic behaviour, on the other hand sample containing both hematite and maghemite phases shows paramagnetic behaviour above 300 K, superparamagnetic behavior at lower temperatures.     

Zinc oxide nanoparticles: a review of their biological synthesis,antimicrobial activity,uptake, translocation and biotransformation in plants

Over the past decade, incorporation of nanomaterials into agricultural practices like nanofertilizers and nanopesticides has gained a lot of attention. Progress and application of fertilizers in nanoforms are one of the effective options for considerable improvement of the agricultural yield worldwide. Zinc oxide nanoparticles (ZnO NPs) are considered as a biosafe material for biological species. Earlier studies have shown the potential of ZnO NPs in stimulation of seed germination and plant growth as well as disease suppression and plant protection by its antimicrobial activity. However, both positive and negative effects of ZnO NPs on plant growth and metabolism at various developmental periods have been documented. Uptake, translocation and accumulation of ZnO NPs by plants depend upon the features of NPs as well as the anatomy of the host plant. This review summarizes the applications of ZnO NPs as nanofertilizer in crop production and also attempts to examine and record the possible mechanism of antimicrobial activity of ZnO NPs. Biological synthesis of ZnO NPs and their uptake, translocation and biotransformation in plants via various routes have also been examined.     

Calcium carbonate nanoparticles: synthesis, characterization and biocompatibility

The synthesis of nanoparticles and their functionalization to effectively utilize them in biological applications including drug delivery is currently a challenge. Calcium carbonate among many other inorganic nanosized particles offers promising results for such applications. We have synthesized calcium carbonate nanoparticles using polymer mediated growth technique, where one of the ions bound within polymer matrix and the other diffuses and reacts to form desired compound. The synthesized nanoparticles are characterized using X-ray diffraction, Scanning Electron Microscopy and spectroscopic techniques such as Fourier-Transform Infra-red spectroscopy and UV-Vis spectroscopy. The diameter of the calcium carbonate nanoparticles is estimated to be 39.8 nm and their biocompatibility studies showed no significant induction of oxidative stress or cell death even at higher concentrations (50 microg) upon exposure to HeLa and LE cells. Here, we report that the synthesized calcium carbonate nanosized particles using polymer mediated growth technique are biocompatible and can be safely used for biomedical applications.     

Hydrothermal synthesis of nickel iron oxide nano-composite and application as magnetically separable photocatalyst for degradation of Solar Blue G dye

In this research, nickel iron oxide nano-composite was effectively prepared via a simple hydrothermal route in an autoclave at 180?°C. The phase formation and opto-elctronic properties of nano-composite were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), UV–Vis diffuse reflectance spectra (UV–Vis DRS) and vibrating sample magnetometer (VSM) techniques. The VSM reults showed magnetization value of 38.25 emu/g. FTIR and XRD results confirmed the formation of cubic NiFe₂O₄ and rhombohedral Fe₂O₃ phases. The results of FESEM and EDAX studies indicate the formation of nickel iron oxide nano-composite with size of 7–10 nm. UV–Visible diffuse reflectance spectra experimental results showed transition energies of 1.66, 2.5 and 3.7 eV. Additionally, the prepared nickel iron oxide nano-composite were used as photocatalyst for for degradation Solar Blue G dye and the results showed good activity and recyclable by applying an appropriate magnetic field. The reuse of the prepared nickel iron oxide nano-composite for removal of Solar Blue G dye water pollutants was attained in five cycles with an average efficiency of 81%.